WO2010037890A1 - Matériaux nanocomposés présentant des propriétés protectrices contre le rayonnement électromagnétique et procédé permettant de les obtenir - Google Patents
Matériaux nanocomposés présentant des propriétés protectrices contre le rayonnement électromagnétique et procédé permettant de les obtenir Download PDFInfo
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- WO2010037890A1 WO2010037890A1 PCT/ES2009/070411 ES2009070411W WO2010037890A1 WO 2010037890 A1 WO2010037890 A1 WO 2010037890A1 ES 2009070411 W ES2009070411 W ES 2009070411W WO 2010037890 A1 WO2010037890 A1 WO 2010037890A1
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- 238000003381 deacetylation reaction Methods 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229920002549 elastin Polymers 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
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- 239000003925 fat Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000012041 food component Nutrition 0.000 description 1
- 239000005428 food component Substances 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
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- 108010050792 glutenin Proteins 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
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- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 description 1
- 229910000271 hectorite Inorganic materials 0.000 description 1
- IUJAMGNYPWYUPM-UHFFFAOYSA-N hentriacontane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC IUJAMGNYPWYUPM-UHFFFAOYSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 239000006194 liquid suspension Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 235000021485 packed food Nutrition 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 229920001470 polyketone Polymers 0.000 description 1
- 238000012667 polymer degradation Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
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- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000003138 primary alcohols Chemical class 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000007870 radical polymerization initiator Substances 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012758 reinforcing additive Substances 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229910000275 saponite Inorganic materials 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- ZLGIYFNHBLSMPS-ATJNOEHPSA-N shellac Chemical compound OCCCCCC(O)C(O)CCCCCCCC(O)=O.C1C23[C@H](C(O)=O)CCC2[C@](C)(CO)[C@@H]1C(C(O)=O)=C[C@@H]3O ZLGIYFNHBLSMPS-ATJNOEHPSA-N 0.000 description 1
- 235000013874 shellac Nutrition 0.000 description 1
- 239000004208 shellac Substances 0.000 description 1
- 229940113147 shellac Drugs 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910021647 smectite Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229940001941 soy protein Drugs 0.000 description 1
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- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 239000005019 zein Substances 0.000 description 1
- 229940093612 zein Drugs 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/44—Products obtained from layered base-exchange silicates by ion-exchange with organic compounds such as ammonium, phosphonium or sulfonium compounds or by intercalation of organic compounds, e.g. organoclay material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/02—Preparation of oxygen
- C01B13/0229—Purification or separation processes
- C01B13/0248—Physical processing only
- C01B13/0259—Physical processing only by adsorption on solids
- C01B13/0281—Physical processing only by adsorption on solids in getters
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Definitions
- the present invention relates to nanocomposite materials with barrier properties to electromagnetic radiation and the development thereof to confer on them the advantageous ability to block or filter radiation, especially infrared and UV-VIS.
- the blocking is obtained through the incorporation of a specific type of nanolamines of natural and / or synthetic clays and which may or may not be intercalated with organic type materials or with organic / inorganic hybrids, which are incorporated into plastic matrices by in-situ polymerization methods.
- these nanocomposite materials have unique properties in that they additionally lead to an improvement in other physical properties of the matrix as a barrier to gases and vapors, improvement in thermal and mechanical properties, fire resistance and active and bioactive properties with minimal impact in transparency and tenacity.
- the present invention relates to the process for the preparation of said materials.
- the present invention relates to the use of the new materials for multisectoral applications.
- nanocomposite material such as an exfoliated or interleaved plate, with a touch structure of nanometric dimensions, comprising intercalated or exfoliated clay dispersed in a polymer matrix, such as an oligomer, a polymer, or a mixture thereof.
- WO / 2001/012678 describes the method of obtaining nanocomposites based on homopolymers and copolymers of polyamide and silicates.
- the physical properties of the prepared nanocomposites exceed those of the no-load polymers.
- nanocomposite materials with improved barrier, physical, mechanical and thermal properties with respect to the improved pure polymer and also with the ability to block electromagnetic radiation and with the additional ability to allow the fixation and / or controlled release of substances active (such as antimicrobials, antioxidants, oxygen sequestrants) and bioactive.
- substances active such as antimicrobials, antioxidants, oxygen sequestrants
- the wavelengths of greatest interest in barrier applications against electromagnetic radiation are mainly between 200 nm and 1 mm.
- This section of the electromagnetic spectrum can be divided into 3 zones: the Ultraviolet (UV) zone between (100-400), the visible zone (400-700 nm) and the near infrared zone (700-2.200 nm).
- UV Ultraviolet
- Other areas of the electromagnetic spectrum of interest in applications are microwaves and radio waves, that is, from 1 mm to 10 km in wavelength.
- Ultraviolet radiation is only 3% of the total radiation received by the earth, but this Radiation is the cause of chemical reactions, degradation of polymers and even discoloration. For this reason, blocking electromagnetic radiation is an important parameter for plastics in multisectoral applications such as food packaging, greenhouse films, coatings in general applications including military and civil applications, spray products, creams and paints and other applications with interest in protection against the penetration of electromagnetic radiation.
- the present invention describes nanocomposites that have electromagnetic radiation barrier properties either globally or selectively, due to the chemical composition thereof, their surface modification and the good dispersion of clay nanolines in the plastic matrix that lead to an absorption, refraction or diffraction of the radiation that passes through the composite material. Due to the small size of the loads, nanometric in thickness, and their high aspect ratio and chemical functionality, their application is advantageous because they additionally lead to synergies in other properties such as the improvement of thermal and gas vapor and vapor barrier properties. or mechanical, and allow the possibility of Ia incorporation of active substances (such as antimicrobials, antioxidants) and bioactive substances and allow the fixation or controlled release of these.
- active substances such as antimicrobials, antioxidants
- nanoadditives are dispersed in a liquid monomer or a mixture of several monomers or a solution or dispersion thereof and then the polymerization is initiated, giving rise to the nanocomposite, for its advantageous application both in the packaging of products of interest for the food and for Applications in other sectors.
- a first essential aspect of the present invention refers to nanocomposite materials comprising at least:
- Lamellar nanoadditives (clay nanolines) with or without organic and / or inorganic surface modification.
- thermoplastic elastomeric, thermostable or polymers derived from biomass and / or biodegradable.
- laminar-type nanoadditives are based mainly on laminar phyllosilicates and / or double laminar hydroxides and / or mixtures of these with each other or with other phyllosilicates, and in all cases with or without superficial organic or inorganic modification.
- These three minerals have in themselves unique properties in acting as a barrier to electromagnetic radiation due to their natural composition and coloration and or their potential functionalization with absorber products and / or blockers of this radiation.
- the laminar nanoadditives will be in a proportion between 0.01 and 98% by weight within the polymer matrix, preferably between 1% and 50%.
- the laminar phyllosilicates are selected and without limitation of the group consisting of montmorillonite, kaolinites, gibsitic, dickitite, nacritic, sepiolite, bentonites, smectite, hectorite, sepiolite, saponite, halloisite, vermiculite, mica, preferably based on vermiculite-type materials, Mica and kaolinite.
- the double laminar hydroxides better known as hydrotalcites or LDH are synthetic or natural laminar structure materials that also fulfill blocking functions. These double hydroxides have positive charges on the surface of the sheet structure and interchangeable anions between the sheets to neutralize the charge. In all cases the sheet materials may or may not be interspersed with organic and / or inorganic type materials.
- a preferred embodiment of the present invention refers to the nanocomposite materials as described above, which comprises laminar nanoadditives with surface modification, said modification being the addition of an initiator of a polymerization reaction.
- the superficial modification when applied, allows the polymerization reaction initiator to be introduced into the laminar nanoadditive, selected from the group consisting of free radicals, cationic compounds, anionic compounds, coordination and / or organometallic compounds and also making them compatible with the components of Ia mixture in which the polymerization reaction takes place.
- the surface modification can also increase the blocking capacity of the electromagnetic radiation of the nanoadditives.
- the plastic matrices are selected without limitation from the group consisting of thermoplastics, thermosets and elastomers such as polyolefins, polyester, polyamides, polyimides, polyketones, polyisocyanates, polysulfones, styrenic plastics, phenolic resins, amidic resins, ureic resins, melamine resins, polyester resins, epoxy resins, polycarbonates, polyvinylpyrrolidones, epoxy resins, polyacrylates, epoxy resins, polyacrylates, epoxy resins, polyacrylates polyurethanes, silicones, aramides, polybutadiene, polyisoprenes, polyacrylonitriles, PVDF, PVA, PVOH, EVOH, PVC, PVDC or biomass derivatives and biodegradable materials such as proteins, polysaccharides, lipids and biopolyesters (PHA, PLA, PCL, etc.) or mixtures of all of these and may contain all types of additives typically added to plastics
- the polymeric matrix will be in a proportion between 2 and 99.99% by weight over the total composite material, preferably from 50% to 99.99%.
- the plastic type matrices contain other substances that act as a barrier to electromagnetic radiation to reinforce the effect, substances to confer fire resistance and / or active or bioactive substances, selected from the group formed by salts, can be added.
- organic and inorganic antimicrobial metals preferably silver, copper, nickel or cobalt
- low molecular weight substances that have an active or bioactive character selected from ethanol, or ethylene, or of the essential oils type (preferably thymol, carvacrol, linalool and mixtures)
- small-sized antimicrobial peptides preferably bacteriocins) natural or obtained by genetic modification (preferably nisins, enterokines, lacticines and lysozyme), or natural or synthetic antioxidants (preferably polyphenols, preferably flavonoids, rosemary extract or other plants and vitamins, preferably ascoric acid Bico or vitamin C), or drugs (antibiotics, anticancer agents, etc.), or enzymes or compounds of bioavailable calcium, or prebiotics (non-digestible
- These materials will be in any case primarily characterized by the introduction into the plastic matrices of laminar type loads with sizes in the range of nanometers in thickness that will be nanoparticular in thickness during in-situ polymerization processes.
- a second essential aspect of the present invention relates to a process for obtaining said materials.
- the incorporation of the nanoadditives to form the nanocomposites takes place through an in situ polymerization type procedure and consists of inserting the initiator system necessary for the polymerization reaction in the interlaminar region of the clay particles, preparing a mixture of the intercalated clays with the initiator system with the monomers and start the polymerization reaction. As the polymer chains grow, they will separate the clay sheets until they are dispersed.
- the present invention describes a process for manufacturing the nanocomposite materials described in the present invention, which comprises the steps of:
- the expanders are preferably selected from the group consisting of DMSO, alcohols, acetates, or water and mixture of the above, which activate the fines by an initial increase in the basal spacing of the sheets and modify the surface characteristics of the clay.
- the penetration of the precursors will be accelerated by the use of temperature, a homogenizer turbulent regime, ultrasound, pressure or mixture of the above.
- the drying of these can be carried out by evaporation in an oven, lyophilization, centrifugation and / or gravimetric processes in solution or turbo-dryers or by atomization.
- the solution of the interleaved precursor can be used, without a previous drying process, as a starting means for the next stage of incorporation of the modifier.
- These precursors are added in an amount from 0.01 to 98%, preferably from 1 to 60%.
- the compounds to be inserted are selected and without limitation from the group formed by PVOH, EVOH and derivatives of the same family, and / or biopolymers such as peptides and natural or synthetic proteins via chemical or genetic modification of microorganisms or plants and natural or synthetic polysaccharides via chemical or genetic modification of microorganisms or plants and polypeptides, lipids and waxes, nucleic acids and polymers of synthetic nucleic acids obtained chemically or by genetic modification of microorganisms or plants, and biodegradable polyesters such as polylactic acid, polylactic-glycolic, adipic acid and derivatives and polydroxyalkanoates, preferably polydroxybutyrate and their copolymers with valeriates.
- biopolymers such as peptides and natural or synthetic proteins via chemical or genetic modification of microorganisms or plants and natural or synthetic polysaccharides via chemical or genetic modification of microorganisms or plants and polypeptides, lipids and waxes, nu
- Biomedical materials such as hydroxyapatites and phosphates of organic salts, phosphonium and quaternary ammonium salts allowed for food contact may also be included - preferably ammonium hexadecyltrimethylammonium bromide, ammonium pentadecafluorooctanoate, bis (2-hydroxyethyl) -2 chloride -hydroxypropyl-3- (dodecyloxy) methylammonium and polyethylene glycol esters with aliphatic monocarboxylic acids (C6-C22) and their ammonium and sodium sulfates- and silanes - preferably 3- aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3- glycidoxypropyltrimethoxysilane, (Gamma) -methacryloxypropyl-trimethoxysilane and tetramethylortosilicate and other particles or nanoparticles with
- the organic material that is intercalated is the EVOH or any material of the same family with molar contents of ethylene preferably less than 48%, and more preferably less than 29%, these are taken to saturation in aqueous medium or in solvents specific alcoholic and mixtures of alcohols and water, more preferably water and isopropanol in proportions in volume of water greater than 50%.
- biopolymers with or without plasticizers, with or without crosslinkers and with or without emulsifiers or surfactants or other nanoadditives are from the group consisting of synthetic and natural polysaccharides (vegetable or animal) such as cellulose and derivatives, carrageenans and derivatives, alginates, dextran, gum arabic and preferably chitosan or any of its natural and synthetic derivatives, more preferably chitosan salts and even more preferably chitosan acetate, and both plant and animal derived proteins and corn proteins (zein), gluten derivatives, such as gluten or its gliadin and glutenin fractions and more preferably gelatin, casein and soy proteins and derivatives thereof, as well as natural or synthetic polypeptides preferably of the elastin type obtained by chemical or modification genetics of microorganisms or plants, lipids such as beeswax, car wax nauba, candelilla wax, shellac and fatty acids and monog
- the degree of deacetylation will preferably be greater than 80% and more preferably greater than 87%.
- the penetration of the precursors will be accelerated by the use of temperature, a homogenizer of turbulent regime, ultrasound, pressure or mixture of the above.
- substances of low molecular weight that have barrier character against the penetration of the electromagnetic radiation considered, of fire resistance will be optionally added and / or active or bioactive in order that they are well intercalated and / or released in a controlled manner giving rise to nanocomposites with active or bioactive capacity.
- the active substances will be ethanol, or ethylene, or of the essential oils type, preferably thymol, carvacrol, linalool and mixtures, or natural antimicrobial peptides (bacteriocins) or obtained by genetic modification, preferably nisins, enterokines, lacticines and lysozyme or nanoparticles metal with natural or synthetic antimicrobial or antioxidant properties, preferably polyphenols, and more preferably flavonoids, rosemary extract and vitamins, preferably ascorbic acid or vitamin C, or drugs (anticancer, antibiotics, etc.), or bioavailable calcium enzymes or compounds.
- bacteriocins natural antimicrobial peptides
- These elements are expected to be fixed or released from the nanocomposite towards the product in a controlled manner (control of the matrix) and exert their active or bioactive role, which can be released from the matrix and that the nanoparticles control the kinetics (control of the nanoadditive) or from both.
- the contents to be added are generally less than 80% by volume of the solution, preferably less than 12% and more preferably less than 8%.
- the penetration of these substances is accelerated by the use of temperature, a homogenizer of turbulent regime, ultrasound, pressure or mixture of the above.
- the molecules or functional groups in the introduced molecules belong to the group of ring opening polymerization initiators for polymerization of lactone monomers, ethylene oxide or cyclic siloxane.
- These initiators may contain functional groups of primary alcohols that can be converted to an alkoxide radical, for example, by reaction with AIEt 3 , which initiates ring opening polymerization.
- the molecules or functional groups of the introduced molecules may also belong to the group of free radical polymerization initiators of unsaturated ethylenic monomers, such as secondary benzyl groups linked to a nitroxide.
- the mentioned molecules may contain an anionic or cationic functional group that allows their adhesion to the clay sheets by ion exchange with anions or cations previously present in the interlaminar space.
- the initiators or catalysts of the polymerization reaction or mixture thereof are selected from the group consisting of unsaturated monomers (containing at least one double bond), or from the group of monomers bearing two or more functional groups; and are added in an amount from 0.01 to
- the mixture can contain all types of additives typically added to plastics to improve its processing or its properties.
- Other products with intrinsic barrier properties to electromagnetic radiation such as titanium dioxide or others to reinforce protection, substances to confer fire resistance and / or complementary and / or bioactive active nouns or / or complementary bioactive assets may also be added in all possible compositions. reinforcement
- the additive concentrate may be subjected to a chemical modification to transform the matrix, for example by a hydrolysis process or others typically applied to polymers derived from chemical modification of other polymers that act as precursors including reactive extrusion.
- the concentrate can be added nanoadditive with substances typically used in plastics processing to improve the processing and / or its properties. Also and optionally, other reinforcing additives of the electromagnetic radiation barrier properties, fire resistance and / or active and / or bioactive properties can be incorporated during this step.
- the nanocomposite materials obtained by the process described in the present invention are used to reinforce the barrier against electromagnetic radiation of plastics in packaging applications in general and food and food components in particular, for greenhouse films, coatings in general applications including military and civil applications, spray products, creams and paints, for biomedical applications such as nanobiocomposites and in pharmaceuticals to optionally release active and / or bioactive principles, such as gas barriers, vapors, solvents and products organic, such as aromas and components of aromas, oils, fats and hydrocarbons, and mixed products of organic and inorganic character, for applications that require biodegradable or compostable character, for active containers that require antimicrobial, antioxidant or other nature that require iera
- active and / or bioactive principles such as gas barriers, vapors, solvents and products organic, such as aromas and components of aromas, oils, fats and hydrocarbons, and mixed products of organic and inorganic character, for applications that require biodegradable or compostable character, for active containers that require antimicrobial, antioxidant or other nature that require ier
- nanoadditive concentrate nanocomposite materials obtained is used as a masterbach in any plastics processing process. It can also act as fire resistant materials.
- Figure 1 is an image obtained by scanning electron microscopy (TEM) in which the main morphologies that can be observed in nanocomposites obtained according to the present invention are presented.
- the image shows us that the clay sheets are exfoliated in the polymer matrix and that they have nanometric sizes in thickness. Note the great aspect ratio (ratio between length and thickness) that the scattered sheets have that guarantees great protection against the passage of electromagnetic radiation and against gases and vapors.
- FIG. 2 shows the UV-VIS spectra obtained with a UV-VIS spectrophotometer.
- This chart shows the spectra of 30 micron films of the highly transparent polylactic acid polymer and its nanocomposite with 10% clay content based on vermiculite and prepared according to Example 1 by in-situ polymerization of lactic acid in the presence of the nanoadditive. It is observed how the introduction of the nanoadditive produces a more intense blockage of UV-Vis radiation. In the ordinate axis, the wavelength (nm) is measured against the% transmission of the bees axis.
- Example 1 Polylactic acid (PLA) films with different contents (1%, 5%, 10% and 20%) of clams of the vermiculite type modified with 40% by mass of hexadecyltrimethylammonium bromide and triethylaluminum (AIEI 3 ) as initiator of the polymerization in a 1: 1 ratio and of a clay (5%) of the modified montmorillonite type with 40% by mass of hexadecyltrimethylammonium bromide and triethylaluminum (AIEI3) in a 1: 1 ratio.
- PHA Polylactic acid
- the modified clay was dispersed in a 0.025 molar solution of lactic acid in tetrahydrofuran (THF) at 7O 0 C in an inert atmosphere.
- THF tetrahydrofuran
- the solvent was removed under reduced pressure conditions.
- In-situ polymerization of lactic acid was carried out at 12O 0 C for 48 hours after the swelling of the clay for 1 hour.
- a 30 micron thick film was formed by melt compression of the resulting nanocomposite.
- Example 2 In another study, the dispersibility of UV-Vis light was demonstrated. For this, on the films of about 30 microns, the absorption capacity of UV-Vis radiation was evaluated by means of a UV-Visible spectrophotometer. While the pure polymer has a transmittance of around 100%, the PLA + 10% clay films allow reducing the transmission of UV light between 83-90%, achieving thus effectively blocking the passage of UV radiation and also a large part of the visible radiation. In the case of the visible zone, radiation can be blocked by up to 65% with an addition of 10% clay content (see Figure 2). This type of clays of vermiculite type properly modified, produce a strong blocking of the light in the region both UV and visible, due to the large nanometric dispersion achieved in the matrix.
- biodegradable nanocomposites of polylactic acid results in the formation of a very interesting packaging material for use, for example in the preservation of foods sensitive to UV-Vis radiation and low molecular weight gases such as oxygen, water vapors and limonene.
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Abstract
La présente invention concerne des matériaux nanocomposés présentant des propriétés protectrices contre le rayonnement électromagnétique, lesquels matériaux comprennent des nano-additifs laminaires présentant ou non une modification superficielle organique et/ou inorganique; et une matrice polymère, un procédé permettant d'obtenir et d'utiliser ces matériaux nanocomposés dans des applications de conditionnement, des films pour serres, des revêtements, etc.
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JP2011529587A JP2012504671A (ja) | 2008-10-01 | 2009-10-01 | 電磁放射線に対する障壁特性を有するナノコンポジット材料およびその製造プロセス |
EP09817322A EP2332885A4 (fr) | 2008-10-01 | 2009-10-01 | Matériaux nanocomposés présentant des propriétés protectrices contre le rayonnement électromagnétique et procédé permettant de les obtenir |
US13/121,766 US20120039975A1 (en) | 2008-10-01 | 2009-10-01 | Nanocomposite materials having electromagnetic-radiation barrier properties and process for obtainment thereof |
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ES200802789A ES2335847B9 (es) | 2008-10-01 | 2008-10-01 | Materiales nanocompuestos con propiedades de barrera a la radiacion electromagnetica y procedimiento para su obtencion |
ESP200802789 | 2008-10-01 |
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US (1) | US20120039975A1 (fr) |
EP (1) | EP2332885A4 (fr) |
JP (1) | JP2012504671A (fr) |
ES (1) | ES2335847B9 (fr) |
WO (1) | WO2010037890A1 (fr) |
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JP2014500366A (ja) * | 2010-12-15 | 2014-01-09 | ザ プロクター アンド ギャンブル カンパニー | 吸水性表面改質されたクレイ結合ポリマー |
JP2014522368A (ja) * | 2011-06-03 | 2014-09-04 | ナノバイオマターズ リサーチ アンド デヴェロップメント,エス.エル. | 多機能性の特性を備えた、金属酸化物に基づくナノ複合体材料 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014500366A (ja) * | 2010-12-15 | 2014-01-09 | ザ プロクター アンド ギャンブル カンパニー | 吸水性表面改質されたクレイ結合ポリマー |
JP2014522368A (ja) * | 2011-06-03 | 2014-09-04 | ナノバイオマターズ リサーチ アンド デヴェロップメント,エス.エル. | 多機能性の特性を備えた、金属酸化物に基づくナノ複合体材料 |
ES2415242R1 (es) * | 2011-12-21 | 2013-07-30 | Nanobiomatters Res & Dev S L | Materiales nanocompuestos activos basados en sales generadoras de so2 y edta y el procedimiento para su obtencion |
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ES2335847A9 (es) | 2016-12-30 |
US20120039975A1 (en) | 2012-02-16 |
ES2335847B1 (es) | 2011-01-25 |
ES2335847B9 (es) | 2016-12-30 |
EP2332885A1 (fr) | 2011-06-15 |
EP2332885A4 (fr) | 2012-03-21 |
ES2335847A1 (es) | 2010-04-05 |
JP2012504671A (ja) | 2012-02-23 |
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